Abstract

An analytical methodology was developed to separate and quantify methylmercury (MeHg) and inorganic mercury by high-performance liquid chromatography (HPLC)–cold vapour atomic fluorescence spectrometry (CV-AFS). The use of UV oxidation of the organic forms of mercury, the tin(II) chloride reduction in acidic medium of mercury and the introduction of a water vapour trap based on H 2SO 4/CaCl 2 resulted in a low detection limit (DL) (10±2 pg, mean value±S.D.). The apparatus was operationally optimised through the modified simplex method leading to an increase of the signal by a factor of 2. The method performance has been tested by determining the MeHg concentration in a sediment certified reference material (CRM) and the results were statistically indistinguishable from the certificate value ( α=0.05) both for the mean value and S.D.

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